CN112863879B - Process method for processing and thinning in medium-high voltage anode aluminum foil - Google Patents
Process method for processing and thinning in medium-high voltage anode aluminum foil Download PDFInfo
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- 239000011888 foil Substances 0.000 title claims abstract description 254
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 221
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 220
- 238000000034 method Methods 0.000 title claims abstract description 63
- 238000012545 processing Methods 0.000 title claims description 21
- 230000007797 corrosion Effects 0.000 claims abstract description 170
- 238000005260 corrosion Methods 0.000 claims abstract description 170
- 238000011282 treatment Methods 0.000 claims abstract description 112
- 238000002791 soaking Methods 0.000 claims description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 79
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 68
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 68
- 238000005406 washing Methods 0.000 claims description 68
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 34
- 229910017604 nitric acid Inorganic materials 0.000 claims description 34
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 30
- 238000004140 cleaning Methods 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 15
- 239000008399 tap water Substances 0.000 claims description 15
- 235000020679 tap water Nutrition 0.000 claims description 15
- 239000000243 solution Substances 0.000 description 193
- 230000000052 comparative effect Effects 0.000 description 15
- 238000004804 winding Methods 0.000 description 14
- 239000003990 capacitor Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
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Abstract
The invention discloses a process method for treating and thinning a medium-high voltage anode aluminum foil, which comprises the steps of pretreatment, primary hole-forming corrosion, intermediate treatment corrosion, secondary hole-expanding corrosion, post-treatment and the like. The method can effectively remove the porous layer on the surface of the finished corrosion foil, not only reduces the excess thickness of the corrosion foil, but also does not reduce the specific volume, and improves the specific volume of the corrosion foil in unit thickness.
Description
Technical Field
The invention belongs to the technical field of electrode foil production, and particularly relates to a process method for processing and thinning a medium-high voltage anode aluminum foil.
Background
The aluminum electrolytic capacitor is an energy storage component widely applied in the electronic and electrical industry, and the anode foil for the aluminum electrolytic capacitor is an energy storage raw material. With the rapid development of electronic information technology, the trend of miniaturization and large-capacity capacitors is more and more obvious, and the attention to green and environmental protection of products is more and more paid, so that the requirement of higher environmental protection is put forward in the pursuit of improving the capacity of the high-voltage anode aluminum foil.
At present, the electrolytic corrosion process of the medium-high voltage anode aluminum foil generally comprises four main steps of pretreatment, holing corrosion, reaming corrosion, post-treatment and the like. The key for obtaining high specific capacitance is that tunnel holes with high density, proper pore size distribution and regular hole length are uniformly distributed on the surface of the medium and high anode pressure aluminum foil. The pretreatment has the effects of removing oil stains, impurities and oxidation films on the surface of the plain foil, improving the surface state and promoting the formation of ordered initial tunnel holes when the aluminum foil is subjected to hole corrosion in the next step. The function of the pitting corrosion is to form initial tunnel holes with a certain number, length and aperture on the surface of the aluminum foil by applying direct current. The reaming corrosion has the effect of further electrifying corrosion or chemical corrosion on the basis of the initial tunnel hole, so that the hole diameter of the tunnel hole is further enlarged and reaches the designed size. The post-treatment is used for eliminating residual metal impurities and aluminum powder on the surface of the aluminum foil and chloride ions in the tunnel holes.
In the etching process, etching the pores is a critical step for determining the specific volume of the etched foil. In actual production, each manufacturer improves the uniformity of hair holes, improves the regularity of the depth of the hair holes, improves the hole density of the hair holes, reduces the number of hair holes, improves the thickness of the optical foil and the like by various means. The simplest and most effective way in industrial production is to increase the specific volume by increasing the thickness of the optical foil, but the residual thickness of the etched foil is increased, which is in contradiction with the miniaturization development of the capacitor. In industrial production, the aluminum foil is processed into corrosion foil, and the thickness of the corrosion foil is reduced by 5-7 μm. Although the prior art has a certain corrosion thinning, the surface of the finished corrosion foil always has a thin skin layer or a porous layer containing a large number of transverse branch holes. The presence of this porous layer affects both the appearance and performance of the etched foil. Therefore, developing a method for effectively removing the porous layer to make the etched foil thinner to a greater extent without excessive thinning to cause a decrease in specific volume is one of the approaches to further increase the capacity and miniaturization of the single-thickness aluminum foil.
Disclosure of Invention
Aiming at the defects, the invention discloses a process method for processing and thinning a medium-high voltage anode aluminum foil, which can effectively remove a porous layer on the surface of a finished corrosion foil, not only reduce the residual thickness of the corrosion foil, but also not reduce the specific volume, and improve the specific volume of the corrosion foil in unit thickness.
The invention is realized by adopting the following technical scheme:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting an aluminum foil into a solution A for soaking treatment, wherein the solution A contains the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid; in the primary direct current hole corrosion, the applied current density is 200-800 mA/cm 2 The time for applying the current is 50-120 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C, wherein the solution C contains the following components in percentage by mass: 1-5% of silicofluoric acid and 1-5% of phosphoric acid; in the intermediate treatment corrosion, the soaking treatment time is 20-100 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percent of 1-10%; the time for applying current in the secondary direct current reaming corrosion is 100-700 s, and the density of the applied current is 50-200 mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for more than one time, then washing the treated aluminum foil with water, and then putting the washed aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 1-10%; in the post-treatment, the soaking time is 50-200 s, and the temperature of the solution E is 50-70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Further, in the step (1), the aluminum foil is soaked in the solution A for 50-200 s, and the temperature of the solution A is 50-90 ℃.
Further, the temperature of the solution B in the step (2) is 65-85 ℃.
Further, the temperature of the solution C in the step (3) is 45-75 ℃.
Further, the temperature of the solution D in the step (4) is 60-80 ℃.
Compared with the prior art, the technical scheme has the following beneficial effects:
the method has simple process and strong controllability, can use thicker standard smooth foil for production, and is more suitable for producing miniaturized capacitors by circularly and repeatedly carrying out intermediate treatment corrosion and secondary hole expanding corrosion, thinning the porous layer on the surface of the corroded foil by utilizing the intermediate treatment corrosion step, achieving the effect of uniformly thinning the corroded foil by circularly and repeatedly treating the corroded foil, and avoiding the situation that the corroded foil is different in thickness, thereby not only improving the hole expanding efficiency and increasing the specific surface area of the aluminum foil, but also effectively removing the porous layer on the surface of the aluminum foil, leading the corroded foil to be thinned to a greater extent, and leading the thickness of the obtained corroded foil to be not increased or only slightly increased, thereby realizing the improvement of the specific volume and the bending of the corroded foil with unit thickness.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. The specific experimental conditions and methods not indicated in the following examples are generally conventional means well known to those skilled in the art.
Example 1:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 74 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 600mA/cm 2 The time for applying the current was 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 60 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 30 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 70 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 600s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) once, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 2:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 74 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 600mA/cm 2 The time for applying the current is 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 60 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 30 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 70 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 600s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) twice, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percent of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 3:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 74 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 600mA/cm 2 The time for applying the current was 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 60 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 30 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, then placing the aluminum foil into a solution D with the temperature of 70 ℃ for secondary direct current electric reaming corrosion,the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 600s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for three times, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 4:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 74 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current pore-forming corrosion, the applied current density is 600mA/cm 2 The time for applying the current was 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 60 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 30 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 70 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 600s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for four times, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 5:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 60 ℃ for soaking for 100s, wherein the solution A contains the following components in percentage by mass: 2% hydrochloric acid, 35% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 75 ℃ for primary direct-current pore-forming corrosion, wherein the solution B contains the following components in percentage by mass: 5% hydrochloric acid, 15% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 400mA/cm 2 The time for applying the current was 65 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 70 ℃, wherein the solution C contains the following components in percentage by mass: 2.5% of silicofluoric acid and 3% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 50 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then putting the aluminum foil into a solution D with the temperature of 65 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percent of 6%; the time of applying current in the secondary direct current reaming corrosion is 500s, and the density of the applied current is 80mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) once, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 2%; in the post-treatment, the soaking time is 80s, and the temperature of the solution E is 65 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 6:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: soaking the aluminum foil in a solution A at the temperature of 70 ℃ for 150s, wherein the solution A contains the following components in percentage by mass: 5% hydrochloric acid, 30% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then placing the aluminum foil into a solution B at the temperature of 80 ℃ for primary direct-current pore-forming corrosion, wherein the solution B contains the following components in percentage by mass: 8% hydrochloric acid, 30% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 500mA/cm 2 The time for applying the current is 100 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 55 ℃, wherein the solution C contains the following components in percentage by mass: 3% of silicofluoric acid and 4% of phosphoric acid; in the intermediate treatment corrosion, the soaking treatment time is 80 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then putting the aluminum foil into a solution D with the temperature of 75 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 1.5%; the time of applying current in the secondary direct current reaming corrosion is 300s, and the density of the applied current is 120mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for three times, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 6%; in the post-treatment, the soaking time is 180s, and the temperature of the solution E is 60 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 7:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 75 ℃ for soaking for 80s, wherein the solution A contains the following components in percentage by mass: 8% hydrochloric acid, 15% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then placing the aluminum foil into a solution B at the temperature of 70 ℃ for primary direct-current pore-forming corrosion, wherein the solution B contains the following components in percentage by mass: 2% hydrochloric acid, 35% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 700mA/cm 2 The time for applying the current was 90 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 65 ℃, wherein the solution C contains the following components in percentage by mass: 4% of silicofluoric acid and 2.5% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 65 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then putting the aluminum foil into a solution D at 65 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percent of 1-10%; the time of applying current in the secondary direct current reaming corrosion is 200s, and the density of the applied current is 180mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) twice, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 8%; in the post-treatment, the soaking time is 120s, and the temperature of the solution E is 55 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 8:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 90 ℃ for soaking for 50s, wherein the solution A contains the following components in percentage by mass: 1% hydrochloric acid, 10% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 85 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 1% hydrochloric acid, 10% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 200mA/cm 2 The time for applying the current was 50 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 75 ℃, wherein the solution C contains the following components in percentage by mass: 1% of silicofluoric acid and 1% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 20 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D at 80 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 1%; the time of applying current in the secondary direct current reaming corrosion is 100s, and the density of the applied current is 50mA/cm 2 ；
(5) And (3) post-treatment: repeating the step (3) to the step (4) for four times, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 1%; in the post-treatment, the soaking time is 50s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Example 9:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 50 ℃ for soaking for 200s, wherein the solution A contains the following components in percentage by mass: 10% hydrochloric acid, 40% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 65 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 10% hydrochloric acid, 40% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 800mA/cm 2 The time for applying the current was 120 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 45 ℃, wherein the solution C contains the following components in percentage by mass: 5% of silicofluoric acid and 5% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 100 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 60 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 10%; the time of applying current in the secondary direct current reaming corrosion is 700s, and the density of the applied current is 200mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for three times, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 10%; in the post-treatment, the soaking time is 200s, and the temperature of the solution E is 50 ℃;
(6) and (5) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning by using pure water, and then drying and winding the etched foil.
Comparative example 1:
the corrosion treatment of the medium-high voltage anode aluminum foil is carried out by adopting a conventional mode, and the corrosion treatment method specifically comprises the following steps:
(1) pretreatment: soaking the aluminum foil in a mixed solution containing 6 mass percent of hydrochloric acid and 25 mass percent of sulfuric acid at the temperature of 80 ℃ for 120 s;
(2) primary pitting corrosion: washing the pretreated aluminum foil with water, and then performing primary direct current perforation corrosion in a mixed solution containing 6% by mass of hydrochloric acid and 25% by mass of sulfuric acid at the temperature of 75 ℃; the applied current density was 550mA/cm 2 The time for pore corrosion treatment is 80 s;
(3) secondary reaming corrosion: washing the aluminum foil subjected to the primary hole forming corrosion, then putting the aluminum foil into a nitric acid solution with the temperature of 70 ℃ and the mass percentage of 3% for secondary direct-current electric reaming corrosion, and applying the current with the density of 95mA/cm 2 The electric reaming treatment time is 600 s;
(4) and (3) post-treatment: and washing the aluminum foil subjected to the second-stage hole expansion, then soaking the aluminum foil in a nitric acid solution with the temperature of 70 ℃ and the mass percentage of 5% for 100s, and then washing the aluminum foil clean with water, drying and storing the aluminum foil.
Comparative example 2:
the corrosion treatment of the medium-high voltage anode aluminum foil is carried out by adopting a conventional mode, and the corrosion treatment method specifically comprises the following steps:
(1) pretreatment: soaking the aluminum foil in a mixed solution containing 6 mass percent of hydrochloric acid and 25 mass percent of sulfuric acid at the temperature of 80 ℃ for 120 s;
(2) primary pitting corrosion: washing the pretreated aluminum foil with water, and then performing primary direct current perforation corrosion in a mixed solution containing 6% by mass of hydrochloric acid and 25% by mass of sulfuric acid at the temperature of 74 ℃; the applied current density was 600mA/cm 2 The time for pore corrosion treatment is 80 s;
(3) secondary reaming corrosion: washing the aluminum foil subjected to the primary hole forming corrosion, then putting the aluminum foil into a nitric acid solution with the temperature of 70 ℃ and the mass percentage of 3% for secondary direct-current electric reaming corrosion, and applying the current with the density of 100mA/cm 2 The electric reaming treatment time is 600 s;
(4) and (3) post-treatment: and washing the aluminum foil subjected to the second-stage hole expansion, then soaking the aluminum foil in a nitric acid solution with the temperature of 70 ℃ and the mass percentage of 5% for 100s, and then washing the aluminum foil clean with water, drying and storing the aluminum foil.
Comparative example 3:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 74 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 600mA/cm 2 The time for applying the current was 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 30 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 200 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 70 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 600s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) once, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percent of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Comparative example 4:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then placing the aluminum foil into a solution B at 74 ℃ for primary direct-current pore-forming corrosion, wherein the solution B contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 600mA/cm 2 The time for applying the current was 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 90 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 300 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 70 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 600s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) once, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Comparative example 5:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 74 ℃ for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current pore-forming corrosion, the applied current density is 600mA/cm 2 The time for applying the current was 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 60 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 30 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 50 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 800s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for three times, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Comparative example 6:
a process method for processing and thinning a medium-high voltage anode aluminum foil comprises the following steps:
(1) pretreatment: putting the aluminum foil into a solution A at the temperature of 80 ℃ for soaking for 120s, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B at the temperature of 74 ℃ for primary direct current hairAnd (3) corroding holes, wherein the solution B contains the following components in percentage by mass: 6% hydrochloric acid, 25% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 600mA/cm 2 The time for applying the current was 80 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C at the temperature of 60 ℃, wherein the solution C contains the following components in percentage by mass: 2% of silicofluoric acid and 2% of phosphoric acid; in the middle treatment corrosion, the soaking treatment time is 30 s;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D with the temperature of 90 ℃ for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percentage of 3%; the time of applying current in the secondary direct current reaming corrosion is 50s, and the density of the applied current is 100mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for three times, then washing the treated aluminum foil with water, and then putting the aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 5%; in the post-treatment, the soaking time is 100s, and the temperature of the solution E is 70 ℃;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, and then drying, winding and corroding the aluminum foil.
Experimental example:
the corrosion foil is obtained by performing treatments such as hole forming, hole expanding and the like on Xinjiang and manufactured polished foils with the thickness of 132 μm according to the methods described in examples 1 to 9 and comparative examples 1 to 6, and then the corrosion foil is prepared according to the electronic industry standard SJ/T1140-2012 of the people's republic of China: 520V formation is carried out by the method in the electrode foil for the aluminum electrolytic capacitor to obtain an aluminum foil product, and the performance of the aluminum foil product is detected, wherein the specific result is shown in Table 1.
TABLE 1 aluminum foil product Performance test results
| Specific volume (μ F/cm) 2 ） | Bend (Hui) | Residual thickness (mum) | Specific volume/residual thickness x 100 | |
| Example 1 | 0.814 | 73 | 125 | 0.651 |
| Example 2 | 0.822 | 74 | 122.5 | 0.671 |
| Example 3 | 0.818 | 74 | 121 | 0.676 |
| Example 4 | 0.821 | 72 | 120 | 0.684 |
| Example 5 | 0.820 | 72 | 122 | 0.672 |
| Example 6 | 0.820 | 73 | 121 | 0.678 |
| Example 7 | 0.819 | 72 | 121 | 0.677 |
| Example 8 | 0.818 | 71 | 122 | 0.670 |
| Example 9 | 0.821 | 71 | 122 | 0.673 |
| Comparative example 1 | 0.788 | 68 | 127 | 0.620 |
| Comparative example 2 | 0.810 | 70 | 127 | 0.638 |
| Comparative example 3 | 0.811 | 70 | 123 | 0.659 |
| Comparative example 4 | 0.811 | 71 | 123 | 0.659 |
| Comparative example 5 | 0.813 | 68 | 124 | 0.656 |
| Comparative example 6 | 0.810 | 68 | 124 | 0.653 |
The detection results show that the thickness of the corrosion foil can be reduced by 2-7 mu m more by the thinning and maintaining of the intermediate treatment process, the specific volume and the bending performance are obviously superior to those of the method in the comparative example 1 or 2, and the specific volume of the unit thickness is improved by 2-5%.
Meanwhile, the invention obtains the corrosion foil with optimal performance by further optimizing the important process parameters of the intermediate treatment corrosion step and the secondary reaming corrosion step, such as the temperature of the solution C used for the intermediate treatment corrosion and the temperature of the solution D used for the secondary reaming corrosion, and the improvement of the performance of the corrosion foil can be influenced by the over-high or over-low temperature control, for example, the corrosion foil obtained by the method according to the comparative examples 3-6 has the advantages of improving the specific volume performance of unit thickness, but not obviously improving the bending performance, and not obtaining the overall improvement of the performance like the corrosion foil obtained by the method.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (4)
1. A process method for processing and thinning a medium-high voltage anode aluminum foil is characterized by comprising the following steps: the method comprises the following steps:
(1) pretreatment: putting an aluminum foil into a solution A for soaking treatment, wherein the solution A contains the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid; in the primary direct current hole corrosion, the applied current density is 200-800 mA/cm 2 The time for applying the current is 50-120 s;
(3) middle treatment corrosion: washing the aluminum foil treated in the step (2) with water, and then soaking in a solution C, wherein the solution C contains the following components in percentage by mass: 1-5% of silicofluoric acid and 1-5% of phosphoric acid; in the intermediate treatment corrosion, the soaking treatment time is 20-100 s; the temperature of the solution C is 45-75 ℃;
(4) secondary reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then placing the aluminum foil into a solution D for secondary direct current electric reaming corrosion, wherein the solution D is a nitric acid solution with the mass percent of 1-10%; the time for applying current in the secondary direct current reaming corrosion is 100-700 s, and the density of the applied current is 50-200 mA/cm 2 ；
(5) And (3) post-treatment: repeating the steps (3) to (4) for more than one time, then washing the treated aluminum foil with water, and then putting the washed aluminum foil into a solution E for soaking treatment, wherein the solution E is a nitric acid solution with the mass percentage of 1-10%; in the post-treatment, the soaking time is 50-200 s, and the temperature of the solution E is 50-70 ℃;
(6) and (5) cleaning the aluminum foil treated in the step (5) with tap water, then cleaning with pure water, and then drying and coiling to obtain the etched foil.
2. The process method for treating and thinning the medium-high voltage anode aluminum foil according to claim 1, characterized in that: in the step (1), the aluminum foil is soaked in the solution A for 50-200 s, and the temperature of the solution A is 50-90 ℃.
3. The process method for processing thinning in the medium-high voltage anode aluminum foil according to claim 1 is characterized in that: the temperature of the solution B in the step (2) is 65-85 ℃.
4. The process method for processing thinning in the medium-high voltage anode aluminum foil according to claim 1 is characterized in that: the temperature of the solution D in the step (4) is 60-80 ℃.
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